Dinuclear terbium (III) coordination polymer and preparation method and application thereof

A technology of coordination polymers and mixed solvents, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of unstudied optical properties and achieve high purity and simple preparation process

Active Publication Date: 2017-06-09
SHANXI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, 2-(2-pyridyl)-1H-imidazole-4,5-dicarboxylic acid complexes based on alkaline earth metals have been successfully prepared, but rare earth metals and 2-(2-pyridyl)-1H The dinuclear terbium complex of -imidazole-4,5-dicarboxylic acid has not been reported yet, and its related optical properties have not been studied

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  • Dinuclear terbium (III) coordination polymer and preparation method and application thereof
  • Dinuclear terbium (III) coordination polymer and preparation method and application thereof
  • Dinuclear terbium (III) coordination polymer and preparation method and application thereof

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Experimental program
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Embodiment 1

[0020] Embodiment 1. Weigh 0.1mmol TbCl 3 ,0.05mmol H 3 PIDC with 0.05mmol H 2 C 2 o 4 Add containing 5ml H 2 O and 5ml ethanol mixed solvent in a 25ml polytetrafluoroethylene tube, adjust the pH to 4 with 0.2mmol / L KOH. Seal the polytetrafluoroethylene tube in a stainless steel reaction kettle, heat it at 160°C for 72 hours, then cool it down naturally, and precipitate a light yellow blocky crystal overnight, wash it with a mixed solvent of water and ethanol at a volume ratio of 1:1, and then wash it with ether After washing and vacuum drying, the calculated yield of 2-(2-pyridyl)-1H-imidazole-4,5-dicarboxylic acid oxalate rare earth dinuclear terbium(III) coordination polymer was 57.5%. Elemental analysis: Theoretical values: C20.63, H 1.85, N 5.16. Experimental values: C 20.70, H 1.82N 5.19.

Embodiment 2

[0021] Example 2.2-(2-pyridyl)-1H-imidazole-4,5-dicarboxylic acid oxalate rare earth dinuclear terbium (III) coordination polymer structure determination: crystal structure determination using Supernova type X-ray single crystal diffractometer , using graphite monochromatized Mo-Kα rays is the incident radiation, with The diffraction points were collected by scanning, and the unit cell parameters were corrected by the least square method. From the difference Fourier electron density map, the crystal structure was solved by the direct method of SHELXL-2014, and corrected by Lorentz and polarization effects. The detailed crystal determination data are shown in Table 1. Crystal structure see figure 1 .

[0022] Table 1 Crystallographic data of the complexes

[0023]

[0024]

Embodiment 3

[0025] Example 3. Powder diffraction: 2-(2-pyridyl)-1H-imidazole-4,5-dicarboxylic acid oxalate rare earth dinuclear terbium (III) coordination polymer X-ray powder diffraction results show that 2-(2 -Pyridyl)-1H-imidazole-4,5-dicarboxylic acid oxalate rare earth dinuclear terbium (III) coordination polymer crystal sample has a uniform phase, and the experimental diffraction pattern is consistent with the powder diffraction pattern simulated based on the crystal structure, see figure 2 .

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Abstract

The invention discloses a dinuclear terbium (III) coordination polymer and a preparation method and application thereof. A chemical formula of the coordination polymer is [Tb2(HPIDC)(C2O4)2(H2O)3.2H2O]n, wherein H3PIDC is 2-(2-pyridyl)-1H-imidazole-4,5-dicarboxylic acid, and H2C2O4 is oxalic acid. The preparation method includes: dissolving TbCl3, H3PyIDC and H2C2O4 into H2O/ethyl alcohol (V:V=1:1) mixed solution according to a molar ratio of 2:1:1, adding KOH solution to adjust pH to 4, and reacting at 160 DEG C for 72h in a hydrothermal reaction kettle; cooling to the room temperature to obtain pale yellow bulk crystals, washing with water and ethyl alcohol mixed solvent, then washing with diethyl ether, and finally performing vacuum drying, wherein the yield is 57.5%. The coordination polymer structurally comprises terbium ions in two coordination modes, ligands are HPIDC<2-> and C2O4<2-> anions, and the dinuclear terbium (III) coordination polymer is a three-dimensional coordination polymer. The coordination polymer is a solid luminescent material, a sample is capable of emitting green light by 330nm-wavelength optical excitation, a chromaticity coordinate is (0.284, 0.523), fluorescence quantum yield is 34.7%, and fluorescence lifetime is 1.32ns.

Description

technical field [0001] The present invention relates to a metal complex, in particular to a 2-(2-pyridyl)-1H-imidazole-4,5-dicarboxylic acid oxalate rare earth dinuclear terbium (III) coordination polymer and a preparation method thereof, and the complex Applications of bit polymers as optical materials. Background technique [0002] Rare earth metal complexes have broad application prospects in the fields of luminescence, catalysis, and biomedicine due to their optical, electrical, and magnetic properties. Among them, rare earth metal organic complexes as photoluminescent materials are compared with traditional inorganic luminescent materials. , due to the unique structure and properties of rare earth ions, they have the advantages of high luminous intensity, pure fluorescent color, low excitation energy, high fluorescent efficiency, and easy solubility in organic media after they are coordinated with organic ligands. Therefore, it is considered to be the most promising ty...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09K11/06
CPCC08G83/008C09K11/06C09K2211/1466C09K2211/182
Inventor 张力杨卢丽萍冯思思
Owner SHANXI UNIV
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